CN111218113B - g-C3N4CNT (carbon nano tube) nano hybrid material modified PPESK (Polytetrafluoroethylene-styrene-ethylene-styrene) lubricating film and preparation method thereof - Google Patents
g-C3N4CNT (carbon nano tube) nano hybrid material modified PPESK (Polytetrafluoroethylene-styrene-ethylene-styrene) lubricating film and preparation method thereof Download PDFInfo
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Abstract
The invention provides a g-C3N4A/CNT nano hybrid material modified PPESK lubricating film and a preparation method thereof belong to the technical field of film material preparation. The invention prepares g-C by calcining urea and CNT3N4the/CNT nano hybrid material is used for modifying the PPESK resin, so that a modified PPESK lubricating film with high performance is prepared. The film prepared by the invention has high strength and toughness, outstanding tribological performance, mild reaction conditions, simple preparation process, easy operation and low cost, and is suitable for large-scale production of the polymer self-lubricating composite film.
Description
Technical Field
The invention belongs to the technical field of membrane material preparation, relates to a polymer-based solid self-lubricating film, and particularly relates to g-C3N4a/CNT nano hybrid material modified PPESK lubricating film and a preparation method thereof.
Background
Poly (aryl ether sulfone ketone) (PPESK) containing a phthalazinone structure is concerned about due to excellent comprehensive performance, but pure PPESK has low bearing capacity and poor wear resistance, and cannot meet the demand of the industrial development which is different day by day on high-performance lubricating materials; for this reason, many scholars have made performance improvements to PPESK, mainly based on the addition of fillers.
In the prior art, the mechanical or tribological properties of PPESK are improved by adding tubular or sheet fillers to the PPESK, butThe addition of a single filler can only improve one aspect of the performance of the material and cannot meet the increasingly wide industrial requirements. Graphite phase carbon nitride (g-C)3N4) It is a planar two-dimensional sheet structure similar to graphene, and in recent years, g-C is used due to its special structure and excellent performance3N4Becomes a research hotspot in the fields of photocatalysis, energy and the like.
Disclosure of Invention
In order to overcome the defect that the material in the prior art is easy to rub and lose, the invention provides g-C3N4The g-C is obtained by calcining urea and CNT to obtain the g-C3N4the/CNT nano hybrid material is used for modifying the PPESK resin, so that the high-performance PPESK lubricating film is prepared.
The invention firstly provides a g-C3N4the/CNT nano hybrid material modified PPESK lubricating film is formed by g-C3N4the/CNT nano hybrid material is formed by modifying PPESK resin.
The invention also provides a g-C3N4The preparation method of the/CNT nano hybrid material modified PPESK lubricating film comprises the following specific steps:
（1）g-C3N4preparation of/CNT nano hybrid material:
weighing urea and CNT, fully grinding, uniformly dispersing, and calcining under the protection of inert atmosphere. Taking out, repeatedly washing with deionized water and alcohol for several times, centrifuging, and drying to obtain g-C3N4the/CNT nano hybrid material.
（2）g-C3N4Preparation of a/CNT nano hybrid material modified PPESK lubricating film:
mixing the g-C prepared in the step (1)3N4Mixing the/CNT nano hybrid material, the PPESK powder and the organic solvent, mechanically stirring, ultrasonically dispersing uniformly, pouring the mixed solution into a mold, and curing and molding to obtain the modified PPESK lubricating film.
Further, in the step (1), the mass ratio of urea to CNT is: 180-250: 1.
Further, the calcination conditions in step (1) are: raising the temperature to 330-350 ℃ within 80-120 min, and keeping the temperature for 80-120 min; then, the temperature is increased to 500-550 ℃ within 60-100 min, and the temperature is kept for 80-150 min.
Further, in the step (2), the using amount ratio of the PPESK powder to the organic solvent is 1 g: 10-30 mL.
Further, the organic solvent is nitrogen Dimethylacetamide (DMA).
Further, g to C in step (2)3N4The mass ratio of the/CNT nano hybrid material to the PPESK is 0.5-2: 100.
Further, in the step (2), the specific method for curing and forming is as follows: heating to 50-70 ℃ within 20-40 min, and keeping the temperature for 6-9 h; and then raising the temperature to 80-100 ℃ within 30-50 min, and preserving the heat for 3-6 h.
The invention has the beneficial effects that:
in the invention, polyarylethersulfone ketone (PPESK) containing phthalazinone biphenyl structure with the advantages of excellent stability, extremely strong corrosion resistance and the like is used as a matrix; adopts two-dimensional layered nano material-graphite phase carbon nitride (g-C) capable of reducing shearing strength of composite material3N4) The antifriction performance of the composite material is improved; the mechanical and abrasion resistance of the material is improved by using the high-toughness Carbon Nano Tube (CNT), so that the composite material has high elastic modulus, high bearing capacity and excellent tribological performance.
The invention synthesizes g-C on the surface of CNT in situ3N4Preparation of g-C3N4the/CNT nano hybrid material can break g-C through heterogeneous nano materials3N4Or the interaction between the CNTs, solves the common problem of easy agglomeration of the nano material, and can give full play to the g-C3N4Lubrication and CNT reinforcement to improve tribological performance of PPESK.
CNT prepared by the invention and g-C3N4Modified by constituent nano-hybrid materialsThe PPESK lubricating film has the advantages of small consumption of nano hybrid materials, good toughness, good antifriction effect, excellent abrasion resistance and the like, also has good mechanical property and outstanding self-lubricating property, and shows excellent tribological property even under the operating conditions of high load and high running speed. The modified PPESK lubricating film prepared by the invention has the hardness of about 215MPa, the elastic modulus of about 3.30GPa, the friction coefficient of about 0.19 and the lowest wear rate of 2.8 multiplied by 10-5mm3Nm, while the pure PPESK film has a hardness of about 170MPa, an elastic modulus of about 1.82GPa, a friction coefficient of about 0.56 and a wear rate of 2.77x10-4mm3in/Nm. Compared with the prior art, the modified PPESK lubricating film has the advantages that all performances are remarkably improved.
Drawings
FIG. 1 shows g-C in example 1 of the present invention3N4And (3) a scanning electron microscope topography of the nano material.
FIG. 2 shows g-C in example 1 of the present invention3N4And (3) a transmission electron microscope topography of the nano material.
FIG. 3 shows g-C in example 4 of the present invention3N4And (3) a transmission electron microscope topography of the/CNT nano hybrid material.
FIG. 4 shows g-C in example 5 of the present invention3N4Fourier transform infrared spectrogram of/CNT nano hybrid material.
FIG. 5 shows g-C in examples 1 and 5 of the present invention3N4And g-C3N4X-ray diffraction pattern of/CNT nano hybrid material.
Detailed Description
The invention will be further described with reference to the following figures and specific examples, but the scope of the invention is not limited thereto.
Example 1 g-C3N4Preparation of
3g of urea are weighed out and ground in a mortar to be mixed evenly. Placing the mixture into an alumina crucible with a cover under the protection of nitrogen, raising the temperature in a gradient way, and calcining the mixture in a tubular furnace, wherein the procedure is as follows: the temperature is raised from room temperature to 350 ℃ in 90 minutes and the temperature is maintained 100 minutes, then the temperature was raised from 350 ℃ to 550 ℃ over 90 minutes and held for 120 minutes. Naturally cooling to room temperature, taking out the calcined product, repeatedly washing with deionized water and alcohol for several times, centrifuging, and drying to obtain g-C3N4And (3) nano materials.
FIGS. 1 and 2 are g-C3N4The appearance images of a scanning electron microscope and a transmission electron microscope of the nano material can clearly show that the prepared g-C3N4The nano material is a transparent and curled two-dimensional thin-layer structure. FIG. 5 is g-C3N4And g-C3N4X-ray diffraction pattern of/CNT nano hybrid material. From the figure, g-C can be seen3N4Two characteristic diffraction peaks are located at 12.7 degrees and 27.5 degrees and are respectively located on the (100) crystal face and the (002) crystal face. Description of g-C3N4And (3) successfully synthesizing the nano-sheet.
Example 2: g-C3N4Preparation of/CNT nano hybrid material
8g of urea and 0.036g of CNT are weighed out and ground in a mortar for uniform mixing. The mixture was placed in a covered alumina crucible under nitrogen blanket, heated up in a gradient and calcined in a tube furnace with the procedure: the temperature was raised from room temperature to 350 ℃ over 120 minutes, held for 90 minutes, and then raised from 350 ℃ to 550 ℃ over 100 minutes, held for 100 minutes. Naturally cooling to room temperature, taking out the calcined product, repeatedly washing with deionized water and alcohol for several times, centrifuging, and drying to obtain g-C3N4the/CNT nano hybrid material.
Example 3:
（1）g-C3N4preparation of/CNT nano hybrid material:
9g of urea and 0.04g of carbon nanotubes are weighed out and ground in a mortar to be uniformly mixed. The mixture was placed in a covered alumina crucible under nitrogen blanket, heated up in a gradient and calcined in a tube furnace with the procedure: the temperature was raised from room temperature to 330 ℃ over 100 minutes, held for 120 minutes, and then from 330 ℃ to 500 ℃ over 90 minutes, held for 110 minutes. Naturally cooling to room temperature, taking out the calcined product, adding deionized water and wineWashing repeatedly for several times, centrifuging, and drying to obtain g-C3N4the/CNT nano hybrid material.
（2）g-C3N4Preparation of a/CNT nano hybrid material modified PPESK lubricating film:
4.0g of the PPESK powder was dissolved in 50mL of DMA organic solvent and mixed by ultrasonic stirring. Then 0.02g of g-C prepared in step (1) was added3N4Mechanically stirring/CNT nano hybrid material powder, ultrasonically dispersing, uniformly mixing, pouring into a mould, putting into a vacuum drying oven, heating in a gradient manner, and curing and molding, wherein the heating procedure is as follows: the temperature was raised from room temperature to 50 ℃ over 20 minutes and held for 7 hours, then from 50 ℃ to 80 ℃ over 40 minutes and held for 5 hours. And finally, naturally cooling to room temperature, and taking out to obtain the modified PPESK lubricating film A.
The mechanical properties of the modified PPESK lubricating film A obtained by the method are tested on three random points on the surface of the material by a nanoindenter (Antonnpa TTX-NHT3, Austria), and the results are averaged. The tribological properties (the couple of the frictional wear test is a 440C steel ball, and the contact mode is ball-disk contact) were measured by a frictional wear tester (MPX-3C), and at least three groups were measured for each sample, and the average was taken. The hardness of the modified PPESK lubricating film A is 201 MPa, the elastic modulus is 3.11 GPa, the friction coefficient is 0.19, and the wear rate is 4.1 multiplied by 10-5mm3/Nm。
FIG. 3 is g-C of preparation3N4The shape of the/CNT nano hybrid material is shown in the figure, and g-C is seen from the figure3N4Successfully grow on the surface of the CNT, and no agglomeration phenomenon occurs.
Example 4:
（1）g-C3N4preparation of/CNT nano hybrid material:
10g of urea and 0.04g of CNT are weighed out and ground in a mortar to be mixed uniformly. The mixture was placed in a covered alumina crucible under nitrogen blanket, heated up in a gradient and calcined in a tube furnace with the procedure: the temperature is raised from room temperature to 340 ℃ within 120 minutes, the temperature is kept for 100 minutes, and then the temperature is raised from 340 ℃ to 520 ℃ within 70 minutesAnd keeping the temperature for 150 minutes. Naturally cooling to room temperature, taking out the calcined product, repeatedly washing with deionized water and alcohol for several times, centrifuging, and drying to obtain g-C3N4the/CNT nano hybrid material.
（2）g-C3N4Preparation of a/CNT nano hybrid material modified PPESK lubricating film:
4.0g of the PPESK powder was dissolved in 70mL of DMA organic solvent and mixed by ultrasonic stirring. Then 0.06g of g-C prepared in step (1) was added3N4Mechanically stirring/CNT nano hybrid material powder, ultrasonically dispersing, uniformly mixing, pouring into a mould, putting into a vacuum drying oven, heating in a gradient manner, and curing and molding, wherein the heating procedure is as follows: the temperature was raised from room temperature to 60 ℃ over 40 minutes and held for 9 hours, and then from 60 ℃ to 90 ℃ over 50 minutes and held for 4 hours. And finally, naturally cooling to room temperature to obtain the modified PPESK lubricating film B.
The hardness, elastic modulus and tribological performance (the couple of the frictional wear test is 440c steel ball, the contact mode is ball-disk contact) of the obtained modified PPESK lubricating film B are measured, and the hardness of the modified PPESK lubricating film B is 215MPa, the elastic modulus is 3.31 GPa, the friction coefficient is 0.21, and the wear rate is 2.8 multiplied by 10-5mm3/Nm。
Example 5:
（1）g-C3N4preparation of/CNT nano hybrid material:
9g of urea and 0.05g of CNT are weighed out and ground in a mortar to mix well. The mixture was placed in a covered alumina crucible under nitrogen blanket, heated up in a gradient and calcined in a tube furnace with the procedure: the temperature was raised from room temperature to 350 ℃ over 80 minutes and held for 90 minutes, and then the temperature was raised from 350 ℃ to 540 ℃ over 90 minutes and held for 120 minutes. Naturally cooling to room temperature, taking out the calcined product, repeatedly washing with deionized water and alcohol for several times, centrifuging, and drying to obtain g-C3N4the/CNT nano hybrid material.
（2）g-C3N4Lubricating film of/CNT nano hybrid material modified PPESKPreparation of the film:
4.0g of the PPESK powder was dissolved in 60mL of DMA organic solvent and mixed by ultrasonic stirring. Then 0.08g of g-C obtained in step (1) was added3N4The preparation method comprises the following steps of (1) mechanically stirring and ultrasonically dispersing/CNT powder, uniformly mixing, pouring into a mold, putting into a vacuum drying oven, carrying out gradient heating, and carrying out curing molding, wherein the heating procedure is as follows: the temperature was raised from room temperature to 70 ℃ over 30 minutes and held for 6 hours, then from 60 ℃ to 100 ℃ over 50 minutes and held for 3 hours. And finally, naturally cooling to room temperature, and taking out to obtain the modified PPESK lubricating film C.
The hardness, elastic modulus and tribological performance (the couple of the frictional wear test is 440C steel ball, the contact mode is ball-disk contact) of the modified PPESK lubricating film C are measured, and the modified PPESK lubricating film C has the hardness of 227 MPa, the elastic modulus of 3.50 GPa, the friction coefficient of 0.17 and the wear rate of 3.1 multiplied by 10-5mm3/Nm。
FIG. 4 is g-C of preparation3N4Fourier transform infrared spectrogram of/CNT nano hybrid material at 800cm-1And 1200--1There are significant infrared absorption bands which are C-containing3N3Typical infrared absorption bands of triazine aromatic ring structure molecules. The g-C produced can be seen from the figure3N4the/CNT contains abundant active functional groups, and the active functional groups are positioned at the positions which can enable the g-C3N4the/CNT and the PPESK matrix have good interfacial chemical bonding interaction, so that the mechanical and tribological properties of the PPESK can be effectively improved.
FIG. 5 is g-C3N4And g-C3N4X-ray diffraction pattern of/CNT nano hybrid material. For g-C3N4the/CNT nano hybrid material has four diffraction peaks at 12.7 degrees, 26 degrees, 27.5 degrees and 42.5 degrees and g-C3N4And the characteristic peak of the CNT is matched. Description of g-C3N4The hybrid nano/CNT material is successfully synthesized.
The modified PPESK lubricating film prepared by the invention has the hardness of about 215MPa and the elastic modulus of3.30GPa or so, friction coefficient of 0.19 or so, and lowest wear rate of 2.8X 10-5mm3Nm, the unmodified PPESK film has a hardness of about 170MPa, an elastic modulus of about 1.82GPa, a friction coefficient of about 0.56, and a wear rate of 2.77X10- 4mm3in/Nm. In contrast, the modified PPESK lubricating films prepared according to the present invention exhibited significant improvements in each property.
The present invention is not limited to the above-described embodiments, and any obvious improvements, substitutions or modifications can be made by those skilled in the art without departing from the spirit of the present invention.
Claims (7)
1. g-C3N4The preparation method of the/CNT nano hybrid material modified PPESK lubricating film is characterized by comprising the following steps:
（1）g-C3N4preparation of/CNT nano hybrid material:
weighing urea and CNT, fully grinding, uniformly dispersing, and calcining under the protection of inert atmosphere; taking out, repeatedly washing with deionized water and alcohol for several times, centrifuging, and drying to obtain g-C3N4a/CNT nano hybrid material;
（2）g-C3N4preparation of a/CNT nano hybrid material modified PPESK lubricating film:
mixing the g-C prepared in the step (1)3N4Mixing a/CNT (carbon nanotube) nano hybrid material, polyarylethersulfone ketone (PPESK) containing a phthalazinone structure and an organic solvent, mechanically stirring, ultrasonically dispersing uniformly, pouring the mixed solution into a mold, and curing and molding to obtain a modified PPESK lubricating film;
the g to C3N4The mass ratio of the/CNT hybrid material to the PPESK is 0.5-2: 100.
2. g-C according to claim 13N4Preparation method of/CNT (carbon nano tube) nano hybrid material modified PPESK (poly (ethylene-propylene-diene styrene)) lubricating filmThe method is characterized in that in the step (1), the mass ratio of the urea to the CNT is as follows: 180-250: 1.
3. g-C according to claim 13N4The preparation method of the/CNT nano hybrid material modified PPESK lubricating film is characterized in that in the step (1), the calcination conditions are as follows: raising the temperature to 330-350 ℃ within 80-120 min, and keeping the temperature for 80-120 min; and then raising the temperature to 500-550 ℃ within 60-100 min, and preserving the heat for 80-150 min.
4. g-C according to claim 13N4The preparation method of the/CNT nano hybrid material modified PPESK lubricating film is characterized in that in the step (2), the dosage ratio of PPESK to organic solvent is 1 g: 10-30 mL.
5. g-C according to claim 43N4The preparation method of the/CNT nano hybrid material modified PPESK lubricating film is characterized in that the organic solvent is N, N-Dimethylacetamide (DMA).
6. g-C according to claim 13N4The preparation method of the/CNT nano hybrid material modified PPESK lubricating film is characterized in that in the step (2), the curing and forming conditions are as follows: heating to 50-70 ℃ within 20-40 min, and keeping the temperature for 6-9 h; and then raising the temperature to 80-100 ℃ within 30-50 min, and preserving the heat for 3-6 h.
7. The modified PPESK lubricating film prepared by the method of any one of claims 1-6, wherein the modified PPESK lubricating film is prepared by filling g-C with polyarylethersulfone ketone containing phthalazinone biphenyl structure as a base material3N4the/CNT nano hybrid material is prepared.
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